# Supplementary Information (SI) for Materials Advances.
# This journal is © The Royal Society of Chemistry 2026

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_calcium_phenylphosphonate_dihydrate
_database_code_depnum_ccdc_archive 'CCDC 2473954'
loop_
_audit_author_name
_audit_author_address
'James B. Orton'
;University of Southampton
United Kingdom
;
_audit_update_record             
;
2025-12-29 deposited with the CCDC.	2025-12-29 downloaded from the CCDC.
;

#2024ncs0378_exp_1414_8_v1.2
#CSD:2473954

_audit_creation_date             2025-05-19
_audit_creation_method           
;
Olex2 1.5
(compiled 2025.04.05 svn.rf049d14d for OlexSys, GUI svn.r7224)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
marca@unica.it
J.B.Orton@soton.ac.uk
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H7 Ca O4 P, H2 O'
_chemical_formula_sum            'C6 H9 Ca O5 P'
_chemical_formula_weight         232.18
_chemical_melting_point          ?
_chemical_oxdiff_formula         C6H9CaO5P
_chemical_oxdiff_usercomment     
'holey carbon coated copper grid, 200 mesh (Agar Scientific), white powder, sample ground between glass slides, grid tapped, cryo transfer @ 175 K (no plunge), coll @ 175 K, CSD: XIMRET'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ca Ca 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_diffrn_oxdiff_scatteringfactors_ed 
'UCLA (2022) https://srv.mbi.ucla.edu/faes/data'
_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   29.5555(17)
_cell_length_b                   10.9536(4)
_cell_length_c                   5.6509(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1829.42(16)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    4244
_cell_measurement_temperature    175(5)
_cell_measurement_theta_max      0.9000
_cell_measurement_theta_min      0.0810
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.000
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11607
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.44.90a (Rigaku Oxford Diffraction, 2025)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'white (bulk)'
_exptl_crystal_colour_primary    ?
_exptl_crystal_density_diffrn    1.686
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       irregular
_exptl_crystal_F_000             361
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.1236
_diffrn_reflns_av_unetI/netI     0.1129
_diffrn_reflns_Laue_measured_fraction_full 0.904
_diffrn_reflns_Laue_measured_fraction_max 0.899
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            6985
_diffrn_reflns_point_group_measured_fraction_full 0.904
_diffrn_reflns_point_group_measured_fraction_max 0.899
_diffrn_reflns_theta_full        0.863
_diffrn_reflns_theta_max         0.900
_diffrn_reflns_theta_min         0.082
_diffrn_ambient_temperature      175(5)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            Rigaku
loop_
_diffrn_frame_id
_diffrn_frame_h
_diffrn_frame_k
_diffrn_frame_l
_diffrn_frame_start_angle
_diffrn_frame_end_angle
_diffrn_frame_scale
1 0.08064 0.01466 -1.00000 -41.250 -41.000 1.466
2 0.07968 0.01424 -1.00000 -41.000 -40.750 1.204
3 0.07872 0.01382 -1.00000 -40.750 -40.500 1.205
4 0.07776 0.01340 -1.00000 -40.500 -40.250 1.237
5 0.07681 0.01298 -1.00000 -40.250 -40.000 1.084
6 0.07587 0.01256 -1.00000 -40.000 -39.750 1.188
7 0.07492 0.01215 -1.00000 -39.750 -39.500 1.132
8 0.07398 0.01174 -1.00000 -39.500 -39.250 1.203
9 0.07304 0.01132 -1.00000 -39.250 -39.000 1.184
10 0.07211 0.01091 -1.00000 -39.000 -38.750 1.230
11 0.07118 0.01050 -1.00000 -38.750 -38.500 1.187
12 0.07025 0.01010 -1.00000 -38.500 -38.250 1.203
13 0.06932 0.00969 -1.00000 -38.250 -38.000 1.265
14 0.06840 0.00928 -1.00000 -38.000 -37.750 1.239
15 0.06748 0.00888 -1.00000 -37.750 -37.500 1.224
16 0.06657 0.00848 -1.00000 -37.500 -37.250 1.290
17 0.06565 0.00808 -1.00000 -37.250 -37.000 1.310
18 0.06474 0.00767 -1.00000 -37.000 -36.750 1.224
19 0.06383 0.00728 -1.00000 -36.750 -36.500 1.329
20 0.06293 0.00688 -1.00000 -36.500 -36.250 1.224
21 0.06202 0.00648 -1.00000 -36.250 -36.000 1.221
22 0.06112 0.00609 -1.00000 -36.000 -35.750 1.205
23 0.06023 0.00569 -1.00000 -35.750 -35.500 1.403
24 0.05933 0.00530 -1.00000 -35.500 -35.250 1.371
25 0.05844 0.00490 -1.00000 -35.250 -35.000 1.242
26 0.05755 0.00451 -1.00000 -35.000 -34.750 1.344
27 0.05666 0.00412 -1.00000 -34.750 -34.500 1.318
28 0.05577 0.00373 -1.00000 -34.500 -34.250 1.331
29 0.05489 0.00334 -1.00000 -34.250 -34.000 1.257
30 0.05401 0.00296 -1.00000 -34.000 -33.750 1.299
31 0.05313 0.00257 -1.00000 -33.750 -33.500 1.353
32 0.05225 0.00219 -1.00000 -33.500 -33.250 1.227
33 0.05138 0.00180 -1.00000 -33.250 -33.000 1.326
34 0.05050 0.00142 -1.00000 -33.000 -32.750 1.261
35 0.04963 0.00103 -1.00000 -32.750 -32.500 1.378
36 0.04876 0.00065 -1.00000 -32.500 -32.250 1.289
37 0.04789 0.00027 -1.00000 -32.250 -32.000 1.343
38 0.04703 -0.00011 -1.00000 -32.000 -31.750 1.381
39 0.04617 -0.00049 -1.00000 -31.750 -31.500 1.455
40 0.04530 -0.00087 -1.00000 -31.500 -31.250 1.278
41 0.04445 -0.00124 -1.00000 -31.250 -31.000 1.272
42 0.04359 -0.00162 -1.00000 -31.000 -30.750 1.225
43 0.04273 -0.00200 -1.00000 -30.750 -30.500 1.272
44 0.04188 -0.00237 -1.00000 -30.500 -30.250 1.314
45 0.04102 -0.00275 -1.00000 -30.250 -30.000 1.241
46 0.04017 -0.00312 -1.00000 -30.000 -29.750 1.313
47 0.03932 -0.00350 -1.00000 -29.750 -29.500 1.348
48 0.03847 -0.00387 -1.00000 -29.500 -29.250 1.441
49 0.03763 -0.00424 -1.00000 -29.250 -29.000 1.393
50 0.03678 -0.00461 -1.00000 -29.000 -28.750 1.299
51 0.03594 -0.00498 -1.00000 -28.750 -28.500 1.276
52 0.03509 -0.00535 -1.00000 -28.500 -28.250 1.292
53 0.03425 -0.00572 -1.00000 -28.250 -28.000 1.261
54 0.03341 -0.00609 -1.00000 -28.000 -27.750 1.373
55 0.03257 -0.00646 -1.00000 -27.750 -27.500 1.425
56 0.03174 -0.00683 -1.00000 -27.500 -27.250 1.458
57 0.03090 -0.00720 -1.00000 -27.250 -27.000 1.373
58 0.03007 -0.00756 -1.00000 -27.000 -26.750 1.503
59 0.02923 -0.00793 -1.00000 -26.750 -26.500 1.528
60 0.02840 -0.00830 -1.00000 -26.500 -26.250 1.330
61 0.02757 -0.00866 -1.00000 -26.250 -26.000 1.395
62 0.02674 -0.00903 -1.00000 -26.000 -25.750 1.475
63 0.02591 -0.00939 -1.00000 -25.750 -25.500 1.432
64 0.02508 -0.00976 -1.00000 -25.500 -25.250 1.479
65 0.02425 -0.01012 -1.00000 -25.250 -25.000 1.488
66 0.02342 -0.01048 -1.00000 -25.000 -24.750 1.457
67 0.02260 -0.01085 -1.00000 -24.750 -24.500 1.414
68 0.02177 -0.01121 -1.00000 -24.500 -24.250 1.480
69 0.02095 -0.01157 -1.00000 -24.250 -24.000 1.490
70 0.02012 -0.01193 -1.00000 -24.000 -23.750 1.481
71 0.01930 -0.01229 -1.00000 -23.750 -23.500 1.479
72 0.01848 -0.01266 -1.00000 -23.500 -23.250 1.512
73 0.01766 -0.01302 -1.00000 -23.250 -23.000 1.454
74 0.01684 -0.01338 -1.00000 -23.000 -22.750 1.448
75 0.01602 -0.01374 -1.00000 -22.750 -22.500 1.411
76 0.01520 -0.01410 -1.00000 -22.500 -22.250 1.436
77 0.01438 -0.01446 -1.00000 -22.250 -22.000 1.451
78 0.01356 -0.01482 -1.00000 -22.000 -21.750 1.481
79 0.01274 -0.01518 -1.00000 -21.750 -21.500 1.438
80 0.01192 -0.01554 -1.00000 -21.500 -21.250 1.460
81 0.01110 -0.01590 -1.00000 -21.250 -21.000 1.519
82 0.01029 -0.01626 -1.00000 -21.000 -20.750 1.426
83 0.00947 -0.01661 -1.00000 -20.750 -20.500 1.411
84 0.00865 -0.01697 -1.00000 -20.500 -20.250 1.440
85 0.00784 -0.01733 -1.00000 -20.250 -20.000 1.494
86 0.00702 -0.01769 -1.00000 -20.000 -19.750 1.465
87 0.00621 -0.01805 -1.00000 -19.750 -19.500 1.515
88 0.00539 -0.01841 -1.00000 -19.500 -19.250 1.576
89 0.00458 -0.01877 -1.00000 -19.250 -19.000 1.555
90 0.00376 -0.01912 -1.00000 -19.000 -18.750 1.544
91 0.00295 -0.01948 -1.00000 -18.750 -18.500 1.547
92 0.00213 -0.01984 -1.00000 -18.500 -18.250 1.566
93 0.00132 -0.02020 -1.00000 -18.250 -18.000 1.540
94 0.00050 -0.02056 -1.00000 -18.000 -17.750 1.589
95 -0.00031 -0.02091 -1.00000 -17.750 -17.500 1.583
96 -0.00113 -0.02127 -1.00000 -17.500 -17.250 1.590
97 -0.00194 -0.02163 -1.00000 -17.250 -17.000 1.585
98 -0.00276 -0.02199 -1.00000 -17.000 -16.750 1.553
99 -0.00357 -0.02235 -1.00000 -16.750 -16.500 1.571
100 -0.00439 -0.02270 -1.00000 -16.500 -16.250 1.558
101 -0.00520 -0.02306 -1.00000 -16.250 -16.000 1.601
102 -0.00602 -0.02342 -1.00000 -16.000 -15.750 1.620
103 -0.00684 -0.02378 -1.00000 -15.750 -15.500 1.627
104 -0.00765 -0.02414 -1.00000 -15.500 -15.250 1.587
105 -0.00847 -0.02450 -1.00000 -15.250 -15.000 1.549
106 -0.00929 -0.02486 -1.00000 -15.000 -14.750 1.567
107 -0.01010 -0.02522 -1.00000 -14.750 -14.500 1.565
108 -0.01092 -0.02558 -1.00000 -14.500 -14.250 1.590
109 -0.01174 -0.02594 -1.00000 -14.250 -14.000 1.662
110 -0.01256 -0.02630 -1.00000 -14.000 -13.750 1.606
111 -0.01338 -0.02666 -1.00000 -13.750 -13.500 1.706
112 -0.01420 -0.02702 -1.00000 -13.500 -13.250 1.634
113 -0.01502 -0.02738 -1.00000 -13.250 -13.000 1.593
114 -0.01584 -0.02774 -1.00000 -13.000 -12.750 1.627
115 -0.01666 -0.02810 -1.00000 -12.750 -12.500 1.603
116 -0.01748 -0.02846 -1.00000 -12.500 -12.250 1.640
117 -0.01831 -0.02882 -1.00000 -12.250 -12.000 1.713
118 -0.01913 -0.02918 -1.00000 -12.000 -11.750 1.600
119 -0.01996 -0.02955 -1.00000 -11.750 -11.500 1.641
120 -0.02078 -0.02991 -1.00000 -11.500 -11.250 1.660
121 -0.02161 -0.03027 -1.00000 -11.250 -11.000 1.673
122 -0.02244 -0.03064 -1.00000 -11.000 -10.750 1.714
123 -0.02326 -0.03100 -1.00000 -10.750 -10.500 1.690
124 -0.02409 -0.03136 -1.00000 -10.500 -10.250 1.645
125 -0.02492 -0.03173 -1.00000 -10.250 -10.000 1.735
126 -0.02575 -0.03209 -1.00000 -10.000 -9.750 1.653
127 -0.02659 -0.03246 -1.00000 -9.750 -9.500 1.643
128 -0.02742 -0.03283 -1.00000 -9.500 -9.250 1.601
129 -0.02825 -0.03319 -1.00000 -9.250 -9.000 1.628
130 -0.02909 -0.03356 -1.00000 -9.000 -8.750 1.632
131 -0.02993 -0.03393 -1.00000 -8.750 -8.500 1.697
132 -0.03076 -0.03430 -1.00000 -8.500 -8.250 1.694
133 -0.03160 -0.03466 -1.00000 -8.250 -8.000 1.652
134 -0.03244 -0.03503 -1.00000 -8.000 -7.750 1.664
135 -0.03328 -0.03540 -1.00000 -7.750 -7.500 1.603
136 -0.03413 -0.03577 -1.00000 -7.500 -7.250 1.681
137 -0.03497 -0.03614 -1.00000 -7.250 -7.000 1.652
138 -0.03582 -0.03652 -1.00000 -7.000 -6.750 1.732
139 -0.03667 -0.03689 -1.00000 -6.750 -6.500 1.715
140 -0.03751 -0.03726 -1.00000 -6.500 -6.250 1.726
141 -0.03836 -0.03764 -1.00000 -6.250 -6.000 1.740
142 -0.03922 -0.03801 -1.00000 -6.000 -5.750 1.662
143 -0.04007 -0.03839 -1.00000 -5.750 -5.500 1.768
144 -0.04093 -0.03876 -1.00000 -5.500 -5.250 1.698
145 -0.04178 -0.03914 -1.00000 -5.250 -5.000 1.745
146 -0.04264 -0.03951 -1.00000 -5.000 -4.750 1.742
147 -0.04350 -0.03989 -1.00000 -4.750 -4.500 1.707
148 -0.04436 -0.04027 -1.00000 -4.500 -4.250 1.764
149 -0.04523 -0.04065 -1.00000 -4.250 -4.000 1.723
150 -0.04609 -0.04103 -1.00000 -4.000 -3.750 1.730
151 -0.04696 -0.04141 -1.00000 -3.750 -3.500 1.721
152 -0.04783 -0.04180 -1.00000 -3.500 -3.250 1.730
153 -0.04870 -0.04218 -1.00000 -3.250 -3.000 1.647
154 -0.04957 -0.04256 -1.00000 -3.000 -2.750 1.688
155 -0.05045 -0.04295 -1.00000 -2.750 -2.500 1.648
156 -0.05133 -0.04333 -1.00000 -2.500 -2.250 1.657
157 -0.05221 -0.04372 -1.00000 -2.250 -2.000 1.626
158 -0.05309 -0.04411 -1.00000 -2.000 -1.750 1.628
159 -0.05397 -0.04450 -1.00000 -1.750 -1.500 1.642
160 -0.05486 -0.04489 -1.00000 -1.500 -1.250 1.569
161 -0.05575 -0.04528 -1.00000 -1.250 -1.000 1.644
162 -0.05664 -0.04567 -1.00000 -1.000 -0.750 1.587
163 -0.05754 -0.04606 -1.00000 -0.750 -0.500 1.601
164 -0.05843 -0.04645 -1.00000 -0.500 -0.250 1.628
165 -0.05933 -0.04685 -1.00000 -0.250 0.000 1.632
166 -0.06023 -0.04725 -1.00000 0.000 0.250 1.642
167 -0.06114 -0.04764 -1.00000 0.250 0.500 1.641
168 -0.06204 -0.04804 -1.00000 0.500 0.750 1.656
169 -0.06295 -0.04844 -1.00000 0.750 1.000 1.699
170 -0.06386 -0.04884 -1.00000 1.000 1.250 1.675
171 -0.06478 -0.04924 -1.00000 1.250 1.500 1.688
172 -0.06570 -0.04965 -1.00000 1.500 1.750 1.687
173 -0.06662 -0.05005 -1.00000 1.750 2.000 1.660
174 -0.06754 -0.05046 -1.00000 2.000 2.250 1.685
175 -0.06846 -0.05086 -1.00000 2.250 2.500 1.731
176 -0.06939 -0.05127 -1.00000 2.500 2.750 1.639
177 -0.07033 -0.05168 -1.00000 2.750 3.000 1.619
178 -0.07126 -0.05209 -1.00000 3.000 3.250 1.663
179 -0.07220 -0.05251 -1.00000 3.250 3.500 1.613
180 -0.07314 -0.05292 -1.00000 3.500 3.750 1.628
181 -0.07409 -0.05333 -1.00000 3.750 4.000 1.682
182 -0.07504 -0.05375 -1.00000 4.000 4.250 1.634
183 -0.07599 -0.05417 -1.00000 4.250 4.500 1.652
184 -0.07694 -0.05459 -1.00000 4.500 4.750 1.630
185 -0.07790 -0.05501 -1.00000 4.750 5.000 1.670
186 -0.07886 -0.05543 -1.00000 5.000 5.250 1.630
187 -0.07983 -0.05586 -1.00000 5.250 5.500 1.628
188 -0.08080 -0.05628 -1.00000 5.500 5.750 1.586
189 -0.08177 -0.05671 -1.00000 5.750 6.000 1.629
190 -0.08275 -0.05714 -1.00000 6.000 6.250 1.656
191 -0.08373 -0.05757 -1.00000 6.250 6.500 1.617
192 -0.08471 -0.05800 -1.00000 6.500 6.750 1.683
193 -0.08570 -0.05844 -1.00000 6.750 7.000 1.655
194 -0.08669 -0.05887 -1.00000 7.000 7.250 1.637
195 -0.08769 -0.05931 -1.00000 7.250 7.500 1.626
196 -0.08869 -0.05975 -1.00000 7.500 7.750 1.701
197 -0.08970 -0.06019 -1.00000 7.750 8.000 1.723
198 -0.09071 -0.06064 -1.00000 8.000 8.250 1.687
199 -0.09172 -0.06108 -1.00000 8.250 8.500 1.701
200 -0.09274 -0.06153 -1.00000 8.500 8.750 1.705
201 -0.09376 -0.06198 -1.00000 8.750 9.000 1.692
202 -0.09479 -0.06243 -1.00000 9.000 9.250 1.635
203 -0.09582 -0.06288 -1.00000 9.250 9.500 1.692
204 -0.09686 -0.06334 -1.00000 9.500 9.750 1.751
205 -0.09790 -0.06380 -1.00000 9.750 10.000 1.764
206 -0.09894 -0.06426 -1.00000 10.000 10.250 1.698
207 -0.09999 -0.06472 -1.00000 10.250 10.500 1.717
208 -0.10105 -0.06518 -1.00000 10.500 10.750 1.718
209 -0.10211 -0.06565 -1.00000 10.750 11.000 1.702
210 -0.10318 -0.06612 -1.00000 11.000 11.250 1.686
211 -0.10425 -0.06659 -1.00000 11.250 11.500 1.681
212 -0.10532 -0.06706 -1.00000 11.500 11.750 1.742
213 -0.10641 -0.06754 -1.00000 11.750 12.000 1.686
214 -0.10749 -0.06801 -1.00000 12.000 12.250 1.713
215 -0.10859 -0.06849 -1.00000 12.250 12.500 1.708
216 -0.10968 -0.06898 -1.00000 12.500 12.750 1.705
217 -0.11079 -0.06946 -1.00000 12.750 13.000 1.721
218 -0.11190 -0.06995 -1.00000 13.000 13.250 1.720
219 -0.11301 -0.07044 -1.00000 13.250 13.500 1.698
220 -0.11414 -0.07093 -1.00000 13.500 13.750 1.669
221 -0.11526 -0.07143 -1.00000 13.750 14.000 1.585
222 -0.11640 -0.07193 -1.00000 14.000 14.250 1.690
223 -0.11754 -0.07243 -1.00000 14.250 14.500 1.639
224 -0.11868 -0.07293 -1.00000 14.500 14.750 1.610
225 -0.11984 -0.07344 -1.00000 14.750 15.000 1.620
226 -0.12100 -0.07395 -1.00000 15.000 15.250 1.597
227 -0.12216 -0.07446 -1.00000 15.250 15.500 1.621
228 -0.12334 -0.07498 -1.00000 15.500 15.750 1.557
229 -0.12451 -0.07550 -1.00000 15.750 16.000 1.567
230 -0.12570 -0.07602 -1.00000 16.000 16.250 1.589
231 -0.12689 -0.07654 -1.00000 16.250 16.500 1.556
232 -0.12810 -0.07707 -1.00000 16.500 16.750 1.558
233 -0.12930 -0.07760 -1.00000 16.750 17.000 1.607
234 -0.13052 -0.07813 -1.00000 17.000 17.250 1.625
235 -0.13174 -0.07867 -1.00000 17.250 17.500 1.646
236 -0.13297 -0.07921 -1.00000 17.500 17.750 1.601
237 -0.13421 -0.07976 -1.00000 17.750 18.000 1.629
238 -0.13546 -0.08030 -1.00000 18.000 18.250 1.630
239 -0.13671 -0.08086 -1.00000 18.250 18.500 1.659
240 -0.13797 -0.08141 -1.00000 18.500 18.750 1.640
241 -0.13924 -0.08197 -1.00000 18.750 19.000 1.766
242 -0.14052 -0.08253 -1.00000 19.000 19.250 1.638
243 -0.14181 -0.08310 -1.00000 19.250 19.500 1.649
244 -0.14311 -0.08367 -1.00000 19.500 19.750 1.744
245 -0.14441 -0.08424 -1.00000 19.750 20.000 1.636
246 -0.14572 -0.08482 -1.00000 20.000 20.250 1.643
247 -0.14705 -0.08540 -1.00000 20.250 20.500 1.634
248 -0.14838 -0.08598 -1.00000 20.500 20.750 1.619
249 -0.14972 -0.08657 -1.00000 20.750 21.000 1.606
250 -0.15107 -0.08717 -1.00000 21.000 21.250 1.586
251 -0.15243 -0.08776 -1.00000 21.250 21.500 1.577
252 -0.15380 -0.08836 -1.00000 21.500 21.750 1.559
253 -0.15518 -0.08897 -1.00000 21.750 22.000 1.473
254 -0.15657 -0.08958 -1.00000 22.000 22.250 1.413
255 -0.15797 -0.09020 -1.00000 22.250 22.500 1.444
256 -0.15938 -0.09082 -1.00000 22.500 22.750 1.409
257 -0.16080 -0.09144 -1.00000 22.750 23.000 1.406
258 -0.16224 -0.09207 -1.00000 23.000 23.250 1.401
259 -0.16368 -0.09271 -1.00000 23.250 23.500 1.330
260 -0.16513 -0.09334 -1.00000 23.500 23.750 1.365
261 -0.16660 -0.09399 -1.00000 23.750 24.000 1.386
262 -0.16808 -0.09464 -1.00000 24.000 24.250 1.362
263 -0.16956 -0.09529 -1.00000 24.250 24.500 1.425
264 -0.17106 -0.09595 -1.00000 24.500 24.750 1.366
265 -0.17258 -0.09662 -1.00000 24.750 25.000 1.434
266 -0.17410 -0.09729 -1.00000 25.000 25.250 1.377
267 -0.17564 -0.09796 -1.00000 25.250 25.500 1.465
268 -0.17719 -0.09864 -1.00000 25.500 25.750 1.431
269 -0.17875 -0.09933 -1.00000 25.750 26.000 1.382
270 -0.18033 -0.10002 -1.00000 26.000 26.250 1.394
271 -0.18192 -0.10072 -1.00000 26.250 26.500 1.405
272 -0.18353 -0.10143 -1.00000 26.500 26.750 1.389
273 -0.18514 -0.10214 -1.00000 26.750 27.000 1.355
274 -0.18677 -0.10286 -1.00000 27.000 27.250 1.367
275 -0.18842 -0.10358 -1.00000 27.250 27.500 1.365
276 -0.19008 -0.10431 -1.00000 27.500 27.750 1.324
277 -0.19176 -0.10505 -1.00000 27.750 28.000 1.287
278 -0.19345 -0.10579 -1.00000 28.000 28.250 1.334
279 -0.19515 -0.10654 -1.00000 28.250 28.500 1.334
280 -0.19688 -0.10730 -1.00000 28.500 28.750 1.348
281 -0.19861 -0.10806 -1.00000 28.750 29.000 1.364
282 -0.20037 -0.10883 -1.00000 29.000 29.250 1.352
283 -0.20214 -0.10961 -1.00000 29.250 29.500 1.386
284 -0.20393 -0.11039 -1.00000 29.500 29.750 1.424
285 -0.20573 -0.11119 -1.00000 29.750 30.000 1.385
286 -0.20756 -0.11199 -1.00000 30.000 30.250 1.397
287 -0.20940 -0.11280 -1.00000 30.250 30.500 1.408
288 -0.21125 -0.11361 -1.00000 30.500 30.750 1.367
289 -0.21313 -0.11444 -1.00000 30.750 31.000 1.346
290 -0.21503 -0.11527 -1.00000 31.000 31.250 1.362
291 -0.21694 -0.11611 -1.00000 31.250 31.500 1.366
292 -0.21888 -0.11696 -1.00000 31.500 31.750 1.294
293 -0.22083 -0.11782 -1.00000 31.750 32.000 1.331
294 -0.22281 -0.11869 -1.00000 32.000 32.250 1.317
295 -0.22480 -0.11957 -1.00000 32.250 32.500 1.318
296 -0.22682 -0.12045 -1.00000 32.500 32.750 1.250
297 -0.22886 -0.12135 -1.00000 32.750 33.000 1.233
298 -0.23092 -0.12226 -1.00000 33.000 33.250 1.199
299 -0.23300 -0.12317 -1.00000 33.250 33.500 1.235
300 -0.23511 -0.12410 -1.00000 33.500 33.750 1.165
301 -0.23724 -0.12503 -1.00000 33.750 34.000 1.150
302 -0.23939 -0.12598 -1.00000 34.000 34.250 1.322
303 -0.24157 -0.12694 -1.00000 34.250 34.500 1.289
304 -0.24377 -0.12790 -1.00000 34.500 34.750 1.165
305 -0.24600 -0.12888 -1.00000 34.750 35.000 1.068
306 -0.24825 -0.12987 -1.00000 35.000 35.250 1.126
307 -0.25053 -0.13088 -1.00000 35.250 35.500 1.135
308 -0.25284 -0.13189 -1.00000 35.500 35.750 1.085
309 -0.25518 -0.13292 -1.00000 35.750 36.000 1.141
310 -0.25754 -0.13395 -1.00000 36.000 36.250 1.117
311 -0.25993 -0.13500 -1.00000 36.250 36.500 1.183
312 -0.26235 -0.13607 -1.00000 36.500 36.750 0.988
313 -0.26480 -0.13715 -1.00000 36.750 37.000 0.970
314 -0.26728 -0.13824 -1.00000 37.000 37.250 0.941
315 -0.26980 -0.13934 -1.00000 37.250 37.500 1.062
316 -0.27234 -0.14046 -1.00000 37.500 37.750 1.061
317 -0.27492 -0.14159 -1.00000 37.750 38.000 0.981
318 -0.27753 -0.14274 -1.00000 38.000 38.250 0.989
319 -0.28017 -0.14390 -1.00000 38.250 38.500 0.993
320 -0.28285 -0.14508 -1.00000 38.500 38.750 1.016
321 -0.28557 -0.14627 -1.00000 38.750 39.000 0.947
322 -0.28832 -0.14748 -1.00000 39.000 39.250 0.981
323 -0.29111 -0.14871 -1.00000 39.250 39.500 0.988
324 -0.29394 -0.14995 -1.00000 39.500 39.750 0.985
325 -0.29681 -0.15121 -1.00000 39.750 40.000 0.942
326 -0.29972 -0.15249 -1.00000 40.000 40.250 0.935
327 -0.30266 -0.15378 -1.00000 40.250 40.500 0.892
328 -0.30566 -0.15510 -1.00000 40.500 40.750 0.899
329 -0.30869 -0.15643 -1.00000 40.750 41.000 0.827
330 -0.31177 -0.15779 -1.00000 41.000 41.250 0.811
331 -0.31489 -0.15916 -1.00000 41.250 41.500 0.775
332 -0.31806 -0.16055 -1.00000 41.500 41.750 0.797
333 -0.32128 -0.16197 -1.00000 41.750 42.000 0.757
334 -0.32455 -0.16340 -1.00000 42.000 42.250 0.728
335 -0.32786 -0.16486 -1.00000 42.250 42.500 0.721
336 -0.33123 -0.16634 -1.00000 42.500 42.750 0.733
337 -0.33465 -0.16784 -1.00000 42.750 43.000 0.688
338 -0.33813 -0.16937 -1.00000 43.000 43.250 0.698
339 -0.34166 -0.17092 -1.00000 43.250 43.500 0.671
340 -0.34525 -0.17250 -1.00000 43.500 43.750 0.630
341 -0.34889 -0.17410 -1.00000 43.750 44.000 0.660
342 -0.35260 -0.17573 -1.00000 44.000 44.250 0.613
343 -0.35637 -0.17738 -1.00000 44.250 44.500 0.589
344 -0.36020 -0.17907 -1.00000 44.500 44.750 0.605
345 -0.36409 -0.18078 -1.00000 44.750 45.000 0.581
346 -0.36806 -0.18252 -1.00000 45.000 45.250 0.522
347 -0.37209 -0.18429 -1.00000 45.250 45.500 0.538
348 -0.37619 -0.18610 -1.00000 45.500 45.750 0.493
349 -0.38037 -0.18793 -1.00000 45.750 46.000 0.531
350 -0.38462 -0.18980 -1.00000 46.000 46.250 0.511
351 -0.38895 -0.19170 -1.00000 46.250 46.500 0.453
352 -0.39336 -0.19364 -1.00000 46.500 46.750 0.491
353 -0.39785 -0.19561 -1.00000 46.750 47.000 0.488
354 -0.40242 -0.19763 -1.00000 47.000 47.250 0.482
355 -0.40709 -0.19967 -1.00000 47.250 47.500 0.452
356 -0.41184 -0.20176 -1.00000 47.500 47.750 0.475
357 -0.41668 -0.20389 -1.00000 47.750 48.000 0.454
358 -0.42162 -0.20606 -1.00000 48.000 48.250 0.482
359 -0.42666 -0.20828 -1.00000 48.250 48.500 0.460
360 -0.43180 -0.21054 -1.00000 48.500 48.750 0.429
361 -0.43705 -0.21284 -1.00000 48.750 49.000 0.471
362 -0.44240 -0.21519 -1.00000 49.000 49.250 0.446
363 -0.44787 -0.21759 -1.00000 49.250 49.500 0.424
364 -0.45345 -0.22005 -1.00000 49.500 49.750 0.448
365 -0.45915 -0.22255 -1.00000 49.750 50.000 0.430
366 -0.46498 -0.22511 -1.00000 50.000 50.250 0.389
367 -0.47093 -0.22773 -1.00000 50.250 50.500 0.393
368 -0.47702 -0.23040 -1.00000 50.500 50.750 0.386
369 -0.48324 -0.23314 -1.00000 50.750 51.000 0.343
370 -0.48961 -0.23594 -1.00000 51.000 51.250 0.365
371 -0.49612 -0.23880 -1.00000 51.250 51.500 0.306
372 -0.50279 -0.24173 -1.00000 51.500 51.750 0.379
373 -0.50961 -0.24473 -1.00000 51.750 52.000 0.300
374 -0.51660 -0.24780 -1.00000 52.000 52.250 0.294
375 -0.52377 -0.25095 -1.00000 52.250 52.500 0.261
376 -0.53111 -0.25418 -1.00000 52.500 52.750 0.270
377 -0.53863 -0.25748 -1.00000 52.750 53.000 0.254
378 -0.54635 -0.26087 -1.00000 53.000 53.250 0.254
379 -0.55426 -0.26435 -1.00000 53.250 53.500 0.203
380 -0.56239 -0.26792 -1.00000 53.500 53.750 0.203
381 -0.57073 -0.27159 -1.00000 53.750 54.000 0.218
382 -0.57930 -0.27535 -1.00000 54.000 54.250 0.189
383 -0.58810 -0.27922 -1.00000 54.250 54.500 0.180
384 -0.59715 -0.28320 -1.00000 54.500 54.750 0.205
385 -0.60646 -0.28729 -1.00000 54.750 55.000 0.141
386 -0.61603 -0.29150 -1.00000 55.000 55.250 0.183
387 -0.62588 -0.29583 -1.00000 55.250 55.500 0.148
388 -0.63603 -0.30029 -1.00000 55.500 55.750 0.161
389 -0.64648 -0.30488 -1.00000 55.750 56.000 0.116
390 -0.65726 -0.30961 -1.00000 56.000 56.250 1.000
391 -0.66837 -0.31450 -1.00000 56.250 56.500 1.000

_diffrn_measured_fraction_theta_full 0.904
_diffrn_measured_fraction_theta_max 0.899
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -41.25  56.50   0.25    0.50    --    0.00   0.00   0.00  391
;
_diffrn_measurement_device       'electron diffractometer'
_diffrn_measurement_device_type  
'XtaLAB Synergy-ED, HyPix-ED, electron source at 200keV'
_diffrn_measurement_method       'continuous rotation electron diffraction'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0012925000
_diffrn_orient_matrix_UB_12      -0.0002674000
_diffrn_orient_matrix_UB_13      -0.0008045000
_diffrn_orient_matrix_UB_21      -0.0041349000
_diffrn_orient_matrix_UB_22      -0.0004442000
_diffrn_orient_matrix_UB_23      0.0002681000
_diffrn_orient_matrix_UB_31      -0.0009809000
_diffrn_orient_matrix_UB_32      0.0022321000
_diffrn_orient_matrix_UB_33      -0.0000464000
_diffrn_oxdiff_ac3_digest_hkl    41abc84d5a52f7ca8f480ea3f4d7424a00508e
_diffrn_oxdiff_digest_od_ed      
;

;
_diffrn_radiation_monochromator  none
_diffrn_radiation_probe          electron
_diffrn_radiation_type           electron
_diffrn_radiation_wavelength     0.0251
_diffrn_source                   'electron gun'
_diffrn_source_type              'JEOL JSM-2300ED, LaB6'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1477
_reflns_number_total             1686
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.44.90a (Rigaku OD, 2025)'
_computing_data_collection       
'CrysAlisPro system (CCD 44.66a 64-bit (release 19-08-2024))'
_computing_data_reduction        'CrysAlisPro 1.171.44.90a (Rigaku OD, 2025)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.072
_refine_ls_extinction_coef       7699(50)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.288
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         1686
_refine_ls_number_restraints     143
_refine_ls_R_factor_all          0.2042
_refine_ls_R_factor_gt           0.1861
_refine_ls_restrained_S_all      1.244
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1855P)²+1.7974P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4445
_refine_ls_wR_factor_ref         0.4528
_refine_special_details          
;
A general thermal restraint is placed upon all atoms within the refinement with additional thermal restraints placed on the aromatic carbon atoms (C1 > C6).
The 1,2 and 1,3 distances of the carbon atoms within the aromatic ring (C1 > C6) have been geometrically restrained and their geometry further retrained to be coplanar.
The locations of all hydrogen atoms have been calculated geometrically and refined using riding models.  Orientation of the uncoordinated water (containing O5) was first allowed to refine freely which then settled into a logical hydrogen bonding network...  
it was then necessary to apply a distance restraint between its hydrogen atom (H5a) and the hydrogen atoms one of the adjacent coordinated water molecule (H5a) to conserve a sensible chemical geometry.
;
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H4A,H4B} of O4
 At 1.5 times of:
  {H5A,H5B} of O5
2. Restrained distances
 H5A-H4B
 -2.1 with sigma of 0.04
 C1-C6 = C6-C5 = C5-C7 = C7-C3 = C3-C2 = C2-C1
 1.39 with sigma of 0.01
 C1-C5 \\sim C6-C7 \\sim C5-C3 \\sim C7-C2 \\sim C3-C1 \\sim C2-C6
 with sigma of 0.02
3. Restrained planarity
 C1, C6, C5, C7, C3, C2
 with sigma of 0.1
4. Uiso/Uaniso restraints and constraints
C1 \\sim C6 \\sim C2 \\sim C3 \\sim C7 \\sim C5: within 2A with sigma of 0.01
and sigma for terminal atoms of 0.02 within 2A
5. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
6.a Free rotating group:
 O5(H5A,H5B)
6.b Secondary CH2 refined with riding coordinates:
 O4(H4A,H4B)
6.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C3(H3), C7(H7), C5(H5)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.51168(17) 0.8656(3) 0.6846(6) 0.0210(12) Uani 1 1 d . . . . .
P1 P 0.5621(2) 0.5703(4) 0.6335(7) 0.0181(14) Uani 1 1 d . . . . .
O1 O 0.5477(3) 0.6944(6) 0.5440(12) 0.0177(19) Uani 1 1 d . . . . .
O2 O 0.5394(3) 0.5279(6) 0.8549(12) 0.0177(19) Uani 1 1 d . . . . .
O3 O 0.5560(4) 0.4807(7) 0.4340(13) 0.030(3) Uani 1 1 d . . . . .
O4 O 0.4612(4) 0.7100(7) 0.8552(12) 0.025(2) Uani 1 1 d . . . . .
H4A H 0.453945 0.644694 0.740194 0.031 Uiso 1 1 calc R U . . .
H4B H 0.432786 0.746154 0.916536 0.031 Uiso 1 1 calc DR U . . .
O5 O 0.3735(5) 0.7880(9) 1.0023(19) 0.046(3) Uani 1 1 d G . . . .
H5A H 0.385380 0.872962 1.042322 0.068 Uiso 1 1 d DG U . . .
H5B H 0.368111 0.747842 1.162706 0.068 Uiso 1 1 d G U . . .
C1 C 0.6214(3) 0.5782(9) 0.7031(14) 0.028(2) Uani 1 1 d D U . . .
C6 C 0.6370(3) 0.5244(9) 0.9104(14) 0.033(2) Uani 1 1 d D U . . .
H6 H 0.613271 0.482154 1.031230 0.040 Uiso 1 1 calc R U . . .
C2 C 0.6523(3) 0.6290(11) 0.5463(16) 0.038(3) Uani 1 1 d D U . . .
H2 H 0.640862 0.663875 0.377305 0.046 Uiso 1 1 calc R U . . .
C3 C 0.6980(4) 0.6354(12) 0.6057(19) 0.048(3) Uani 1 1 d D U . . .
H3 H 0.721358 0.684413 0.492567 0.057 Uiso 1 1 calc R U . . .
C7 C 0.7136(4) 0.5788(13) 0.8099(18) 0.050(3) Uani 1 1 d D U . . .
H7 H 0.749490 0.577009 0.849340 0.060 Uiso 1 1 calc R U . . .
C5 C 0.6828(3) 0.5245(11) 0.9632(17) 0.044(3) Uani 1 1 d D U . . .
H5 H 0.694679 0.482116 1.124831 0.053 Uiso 1 1 calc R U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ca1 O1 2.298(8) . ?
Ca1 O1 2.385(8) 7_576 ?
Ca1 O2 2.342(10) 3_656 ?
Ca1 O2 2.345(8) 7_575 ?
Ca1 O3 2.556(10) 7_576 ?
Ca1 O4 2.463(10) . ?
Ca1 O4 2.526(9) 7_575 ?
P1 O1 1.512(9) . ?
P1 O2 1.495(9) . ?
P1 O3 1.506(9) . ?
P1 C1 1.798(11) . ?
O4 H4A 0.9900 . ?
O4 H4B 0.9900 . ?
O5 H5A 1.0200 . ?
O5 H5B 1.0199 . ?
C1 C6 1.390(8) . ?
C1 C2 1.389(8) . ?
C6 H6 1.0830 . ?
C6 C5 1.386(9) . ?
C2 H2 1.0830 . ?
C2 C3 1.393(9) . ?
C3 H3 1.0830 . ?
C3 C7 1.389(9) . ?
C7 H7 1.0830 . ?
C7 C5 1.391(9) . ?
C5 H5 1.0830 . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Ca1 O1 82.1(3) . 7_576 ?
O1 Ca1 O2 152.2(3) . 3_656 ?
O1 Ca1 O2 88.3(3) . 7_575 ?
O1 Ca1 O3 58.9(3) 7_576 7_576 ?
O1 Ca1 O3 119.4(4) . 7_576 ?
O1 Ca1 O4 75.3(3) 7_576 . ?
O1 Ca1 O4 143.2(3) 7_576 7_575 ?
O1 Ca1 O4 81.4(3) . . ?
O1 Ca1 O4 75.6(3) . 7_575 ?
O2 Ca1 O1 131.2(4) 7_575 7_576 ?
O2 Ca1 O1 125.3(3) 3_656 7_576 ?
O2 Ca1 O2 76.8(3) 3_656 7_575 ?
O2 Ca1 O3 86.1(3) 7_575 7_576 ?
O2 Ca1 O3 83.3(3) 3_656 7_576 ?
O2 Ca1 O4 77.5(3) 7_575 7_575 ?
O2 Ca1 O4 99.9(4) 3_656 . ?
O2 Ca1 O4 150.1(3) 7_575 . ?
O2 Ca1 O4 78.3(3) 3_656 7_575 ?
O4 Ca1 O3 123.4(3) . 7_576 ?
O4 Ca1 O3 157.7(3) 7_575 7_576 ?
O4 Ca1 O4 72.7(3) . 7_575 ?
Ca1 P1 Ca1 95.34(18) 7_575 3_646 ?
O1 P1 Ca1 51.1(3) . 7_575 ?
O1 P1 Ca1 122.0(5) . 3_646 ?
O1 P1 C1 107.8(6) . . ?
O2 P1 Ca1 39.5(4) . 3_646 ?
O2 P1 Ca1 123.5(5) . 7_575 ?
O2 P1 O1 115.6(5) . . ?
O2 P1 O3 111.7(6) . . ?
O2 P1 C1 105.7(5) . . ?
O3 P1 Ca1 57.6(4) . 7_575 ?
O3 P1 Ca1 73.1(4) . 3_646 ?
O3 P1 O1 107.6(5) . . ?
O3 P1 C1 108.2(6) . . ?
C1 P1 Ca1 130.7(3) . 7_575 ?
C1 P1 Ca1 127.6(3) . 3_646 ?
Ca1 O1 Ca1 108.3(4) . 7_575 ?
P1 O1 Ca1 138.5(5) . . ?
P1 O1 Ca1 99.4(4) . 7_575 ?
Ca1 O2 Ca1 103.2(3) 3_646 7_576 ?
P1 O2 Ca1 116.5(5) . 3_646 ?
P1 O2 Ca1 131.8(4) . 7_576 ?
P1 O3 Ca1 92.6(4) . 7_575 ?
Ca1 O4 Ca1 99.0(4) . 7_576 ?
Ca1 O4 H4A 112.0 . . ?
Ca1 O4 H4A 112.0 7_576 . ?
Ca1 O4 H4B 112.0 . . ?
Ca1 O4 H4B 112.0 7_576 . ?
H4A O4 H4B 109.6 . . ?
H5A O5 H5B 104.5 . . ?
C6 C1 P1 119.1(6) . . ?
C2 C1 P1 121.4(6) . . ?
C2 C1 C6 119.3(7) . . ?
C1 C6 H6 119.8 . . ?
C5 C6 C1 120.3(7) . . ?
C5 C6 H6 119.8 . . ?
C1 C2 H2 119.9 . . ?
C1 C2 C3 120.3(7) . . ?
C3 C2 H2 119.9 . . ?
C2 C3 H3 120.0 . . ?
C7 C3 C2 120.0(8) . . ?
C7 C3 H3 120.0 . . ?
C3 C7 H7 120.3 . . ?
C3 C7 C5 119.4(8) . . ?
C5 C7 H7 120.3 . . ?
C6 C5 C7 120.4(7) . . ?
C6 C5 H5 119.8 . . ?
C7 C5 H5 119.8 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O4 H4A O3 0.99 1.71 2.700(11) 173.0 5_666 yes
O4 H4B O5 0.99 1.88 2.852(18) 168.5 . yes
O5 H5A O3 1.02 2.10 2.988(16) 144.1 3_656 yes
O5 H5B O5 1.02 1.97 2.946(5) 160.3 7_576 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ca1 P1 O1 Ca1 131.7(11) 7_575 . . . ?
Ca1 P1 O1 Ca1 63.0(9) 3_646 . . . ?
Ca1 P1 O1 Ca1 -68.7(4) 3_646 . . 7_575 ?
Ca1 P1 O2 Ca1 51.2(6) 7_575 . . 3_646 ?
Ca1 P1 O2 Ca1 -91.0(8) 7_575 . . 7_576 ?
Ca1 P1 O2 Ca1 -142.1(10) 3_646 . . 7_576 ?
Ca1 P1 O3 Ca1 107.9(4) 3_646 . . 7_575 ?
Ca1 P1 C1 C6 -169.5(6) 7_575 . . . ?
Ca1 P1 C1 C6 -24.6(10) 3_646 . . . ?
Ca1 P1 C1 C2 5.8(12) 7_575 . . . ?
Ca1 P1 C1 C2 150.7(8) 3_646 . . . ?
P1 C1 C6 C5 177.2(9) . . . . ?
P1 C1 C2 C3 179.2(10) . . . . ?
O1 P1 O2 Ca1 109.9(6) . . . 3_646 ?
O1 P1 O2 Ca1 -32.2(10) . . . 7_576 ?
O1 P1 O3 Ca1 -11.0(7) . . . 7_575 ?
O1 P1 C1 C6 137.0(8) . . . . ?
O1 P1 C1 C2 -47.7(10) . . . . ?
O2 P1 O1 Ca1 -113.6(6) . . . 7_575 ?
O2 P1 O1 Ca1 18.2(11) . . . . ?
O2 P1 O3 Ca1 116.8(5) . . . 7_575 ?
O2 P1 C1 C6 12.8(9) . . . . ?
O2 P1 C1 C2 -171.9(9) . . . . ?
O3 P1 O1 Ca1 143.7(8) . . . . ?
O3 P1 O1 Ca1 12.0(7) . . . 7_575 ?
O3 P1 O2 Ca1 -13.5(8) . . . 3_646 ?
O3 P1 O2 Ca1 -155.6(7) . . . 7_576 ?
O3 P1 C1 C6 -107.0(8) . . . . ?
O3 P1 C1 C2 68.3(10) . . . . ?
C1 P1 O1 Ca1 128.5(4) . . . 7_575 ?
C1 P1 O1 Ca1 -99.8(9) . . . . ?
C1 P1 O2 Ca1 86.9(8) . . . 7_576 ?
C1 P1 O2 Ca1 -130.9(5) . . . 3_646 ?
C1 P1 O3 Ca1 -127.2(4) . . . 7_575 ?
C1 C6 C5 C7 0.2(14) . . . . ?
C1 C2 C3 C7 7(2) . . . . ?
C6 C1 C2 C3 -5.5(17) . . . . ?
C2 C1 C6 C5 1.8(13) . . . . ?
C2 C3 C7 C5 -5(2) . . . . ?
C3 C7 C5 C6 1.4(18) . . . . ?


_olex2_date_sample_data_collection 2024-08-21
_olex2_date_sample_submission    2024-05-24
_olex2_exptl_crystal_mounting_method 
'The crystal was mounted on a Agar lacey carbon grid'
_olex2_submission_original_sample_id MicroED0-02
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 13.950
_oxdiff_exptl_absorpt_empirical_full_min 0.502
_diffrn_ambient_environment      vacuum
_diffrn_source_details           LaB6
_diffrn_source_voltage           200
_diffrn_measurement_specimen_support 
'holey carbon coated copper grid, 200 mesh (Agar Scientific); Gatan Elsa cryo-transfer holder 698'
_exptl_special_details           
'Gatan Elsa cryo-transfer holder model 698. Temperature controller model 1905'
_exptl_crystal_preparation       
'Sample ground between glass slides, grid dabbed, cryo transfer @ 175 K'
_exptl.crystals_number           1
_diffrn_source.description       'electron gun'
_diffrn_source.make              LaB6
_diffrn_source.ed_diffracting_area_selection SAED
_diffrn_detector.description     'Hybrid Pixel Array Detector'
_diffrn_detector.make            'Rigaku HyPix-ED'
_diffrn_measurement.rotation_mode rotation
_refine.diffraction_theory       kinematical
_diffrn_measurement.method_precession no


_vrf_PLAT029_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.904 Why?  
RESPONSE: Data completeness was limited by the angular range of the 3D Electron
 Diffraction (3DED) instrument.  This may be overcome by merging data from 
several comparable particles, however this approach can suffer from the 
constituent datasets being subject to the effects inherent to 3DED, e.g. high 
vacuum, radiation damage and dynamical scattering; and each potentially by 
differing extents. For this sample, the best model refinement was obtained 
from non-merged data, collected from a single particle: with the data 
resolution truncated to 0.8A, the 10 of the most disagreeable reflections 
(I(obs) and I(calc) differ >10 times SigmaW) omitted from the refinement, 
and all frames outside the range of -41.25deg. \w to +56.5deg. \w (from total 
possible range of -61.0deg. \w to +59.75deg. \w) due to full or partial 
occlusion of the diffracted electrons by the sample grid.
;
_vrf_PLAT921_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: R1 in CIF and R1 Calcd from FCF Data Differ by .    -0.6229 Check 
RESPONSE: This alert this alert has been reviewed and was found to be 
erroneous.  There is an issue with the current version of checkCIF and 3D 
Electron Diffraction (3DED) output from ShelXL (2018/3). This case is under 
discussion (circa Dec. 2025) with the IUCr, so that it may be resolved in 
future versions of checkCIF. 
;
_vrf_PLAT922_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: wR2 in the CIF and FCF Differ by ...............    -0.4982 Check 
RESPONSE: This alert this alert has been reviewed and was found to be 
erroneous.  There is an issue with the current version of checkCIF and 3D 
Electron Diffraction (3DED) output from ShelXL (2018/3). This case is under 
discussion (circa Dec. 2025) with the IUCr, so that it may be resolved in 
future versions of checkCIF.
;
_vrf_PLAT923_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: S    Values in the CIF and FCF Differ by .......     -4.659 Check 
RESPONSE: This alert this alert has been reviewed and was found to be 
erroneous.  There is an issue with the current version of checkCIF and 3D 
Electron Diffraction (3DED) output from ShelXL (2018/3). This case is under 
discussion (circa Dec. 2025) with the IUCr, so that it may be resolved in 
future versions of checkCIF.
;
_vrf_PLAT934_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: Number of (Iobs-Icalc)/Sigma(W) > 10 Outliers ..         24 Check 
RESPONSE: This alert this alert has been reviewed and was found to be 
erroneous.  There is an issue with the current version of checkCIF and 3D 
Electron Diffraction (3DED) output from ShelXL (2018/3). This case is under 
discussion (circa Dec. 2025) with the IUCr, so that it may be resolved in 
future versions of checkCIF.
;
_vrf_PLAT973_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: Check Calcd Positive Resid. Density on       Ca1       2.70 eA-3  
RESPONSE: This alert this alert has been reviewed and was found to be 
erroneous.  This flagged positive residual density peak is not found in the 
refined model and results from an issue with the current version of checkCIF 
and 3D Electron Diffraction (3DED) output from ShelXL (2018/3). This case is 
under discussion (circa Dec. 2025) with the IUCr, so that it may be resolved 
in future versions of checkCIF.
;
_vrf_PLAT082_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: High R1 Value ..................................       0.19 Report
RESPONSE: Dynamical effects arising from multiple scattering, radiation and 
vacuum damage all contribute to relatively high R1 values for structures 
derived from 3DED. The effects of these were minimised by using data from 
a single particle/scan and rigorous scaling procedures. The structure was 
refined using a kinematic approximation and further accounting for dynamical 
effects was not deemed necessary. An R1 value of c.a. 19% is common for 3DED 
derived structures and represents a trustworthy model which is sufficient for 
confirmation of the structure and provides suitably accurate derive geometry.
;
_vrf_PLAT084_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: High wR2 Value (i.e. > 0.25) ...................       0.45 Report
RESPONSE: Dynamical effects arising from multiple scattering, radiation and 
vacuum damage all contribute to relatively high R1 values for structures 
derived from 3DED. The effects of these were minimised by using data from 
a single particle/scan and rigorous scaling procedures. The structure was 
refined using a kinematic approximation and further accounting for dynamical 
effects was not deemed necessary. An wR2 value of c.a. 45% is common for 3DED 
derived structures and represents a trustworthy model which is sufficient for 
confirmation of the structure and provides suitably accurate derive geometry.
;
_vrf_PLAT911_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600        107 Report
RESPONSE: This alert this alert has been reviewed found to be erroneous.  The 
best refinement for this data was found by truncating it to 0.8A, with the 
following 10 most disagreeable reflections manually omitted (0 2 0, 0 2 1, 
0 4 0, 0 4 1, 1 3 2, 2 1 1, 3 0 2, 3 3 1, 4 0 2 and 4 2 2).  The current 
version of checkCIF is however falsely flagging reflections beyond 0.8A 
resolution as missing.  This issue with 3D Electron Diffraction (3DED) 
output from ShelXL (2018/3) is under discussion (circa Dec. 2025) with the 
IUCr, so that it may be resolved in future versions of checkCIF.
;
_vrf_PLAT920_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: Theta(Max)  in CIF and FCF Differ by ...........       3.56 Degree
RESPONSE: This alert this alert has been reviewed and was found to be 
erroneous.  There is an issue with the current version of checkCIF and 3D 
Electron Diffraction (3DED) output from ShelXL (2018/3). This case is under 
discussion (circa Dec. 2025) with the IUCr, so that it may be resolved in 
future versions of checkCIF.
;
_vrf_PLAT925_calcium_phenylphosphonate_dihydrate 
;
PROBLEM: The Reported and Calculated Rho(max) Differ by .       2.28 eA-3  
RESPONSE: This alert this alert has been reviewed and was found to be 
erroneous.  There is an issue with the current version of checkCIF and 3D 
Electron Diffraction (3DED) output from ShelXL (2018/3). This case is under 
discussion (circa Dec. 2025) with the IUCr, so that it may be resolved in 
future versions of checkCIF.
;
